反应详情

Phenethylamine (7.0 g, 58.4 mmol) was added to a stirred solution of 2,6-dichloro-9-tetrahydro-2H-pyran-2-yl-9H-purine (14.5 g, 53.1 mmol) (preparation 5) and triethylamine (21 g, 212.5 mmol) in acetonitrile (200 ml). The reaction mixture was stirred for 3 hr at room temperature and then more phenethylamine (1 g, 8.3 mmol) was added. The reaction mixture was stirred for a further 1 hr and then the solvent was removed under reduced pressure to give a residue which was partitioned between diethyl ether (500 ml) and water (250 ml). The diethyl ether layer was washed with more water (300 ml). The solvent was removed from the organic phase under reduced pressure to give a residue which was purified by column chromatography on silica gel eluting with diethyl ether to give the title compound (17.9 g) as a white solid.

1. stirringThe reaction mixture was stirred for a further 1 hr
2. customthe solvent was removed under reduced pressure
3. customto give a residue which
4. customwas partitioned between diethyl ether (500 ml) and water (250 ml)
5. washThe diethyl ether layer was washed with more water (300 ml)
6. customThe solvent was removed from the organic phase under reduced pressure
7. customto give a residue which
8. customwas purified by column chromatography on silica gel eluting with diethyl ether